Impregnated material



ounce STATES PATENT omen.

WINTWORTH V. LANDER, 0F NEWTON, MASSACHUSETTS, ASSIGNOR TO GENERALINDURATING CORPORATION, OF NEW YORK, N. Y., A CORPORATION OF NEW YORK.

IMPREGN'ATED MATERIAL.

No Drawing. Application filedfl'uly 31,

To all whom it may concern:

Be it known that I, WINTWORTH V. LAN- nnn, citizen of the United Statesof America, and resident of Newton, in the county of Middlesex and Stateof Massachusetts, have invented new and useful Improvements inImpregnated Materials, of which the following is a specification.

This invention relates to porous materials impregnated with acomposition comprising crude petrolatum or other suitable petroleumresidue such as described and claimed in my Patents ilo. 1,277,322,granted August 2?, 918, and No. 1,278,943. granted September 4', 1918,of which this is in part a coninuation.

The substances or materials whichare susceptible of impregnation toproduce the improved articles embodying the present inven- 'tion areexemplified by compressed woodpalp articles. such as pulp-boards, pails,toilet seats, etc, and also by flexible sheet materials such as paper,textiles, paper board, leather board and leather, all of which arecharacterized by interstitial structure capable of taking up a liquid bycapillary absorption. Interstitial or porous structure connotes a degreeof structural discontinuity; the impregnation of such a structure with asubstance which in whole or in part fills the interstices or poresincreases or enhances the structural continuity of the body as a whole,by substituting for the gaseous content of the interstices or pores aviscous or solid content, according to the physical character of thefilling material.

One of the main objects of my invention is to render porous or bibulousbodies impervious or resistant to water by reason of the increased orenhanced internalstructural continuity imparted to such bodies by my newcomposition, and this property 18 common to all such bodies afteradequate treatmentby my process and composition. In other respects thequality of porous or bibulous bodies so treated is susceptible of va-"riation in response to variation in the proportions of the ingredientsof the composition and in the method of treatment with the composition.I i The impregnating composition which I employ in producing theimproved articles or products claimed herein comprises a petroleumresidue and a resin, preferably colophony, dissolved in gasolene orsuitable Specification of Letters Patent.

described in said application the crude petrolatum is obtained fromparaffin-base petroleum such as obtained in Pennsylvania, when refinedby the process known as fractional distillation. It has a flash point ofapproximately 500 F., and melting point of the order of 120 to 130 F,and is a mixture of saturated and unsaturated hydrocarbons. The productcomprises olefins, naphthenes and paraiiins in amorphorous form, butcontains no parafiin as such, that is, no parafiin in crystallinecommercial form. Most of the paraffin is removed from the petroleum inthe form of parafiin wax before the crude petrolatum is arrived at. Bothresin and the crude petrolatum are inherently water-resistantsubstances; the gasolene constitutes a vehicle or carrier whichreadilypenetrates the pores of a porous body, carrying into it thewater-resistant ingredients, and depositing them therein by subsequentvolatilization or evaporation.

The functionally valuable characteristics 4 of a carrier of thewater-resistant ingredients are, that it shall be a solvent of the saidingredients or a liquid capable of sustaining them. in a condition ofextension, shall be capable of wetting the substance of which a porousbody to be treated is composed, and shall be volatile or evaporable, soas to leave the ingredients carried into the porous or bibulous body,lodged in the pores or interstices of the-same after treatment.

I am aware that compositions containing a resin and-an asphalt, a resinand paraflin, and an oil dissolved in a volatile carrier, have beensuggested for the purpose of impregnating and Waterproofing porousbodies such as wood-pulp articles or paper board, and that the functionof the volatile carrier insuch cases is the same in substance as that ofthe carrier in my new composition of matter. But none of the proposedcompositions of matter, so far as I am informed or have been able toascertain by observation and experiment, has possessed the range ofapplication, or has been capable of producing ing the products hereinclaimed. Whether the carrier be gasolene or some other volatile orevaporable liquid which may answer the purpose in a measurable degree,or whether common rosin or some other resin be used as the resinousingredient, the employement of crude petrolatum or other suitablepetroleum residue such as described in said applications renders thecomposition capable of securing new and useful results and susceptible,moreover, of producing a wide variety of results and physicalcharacteristics in product, provided the proportions of theWater-resistant ingredients be varied.

A series of practical demonstrations has shown that a composition,characterized by the presence of crude petrolatum and aresln, andintroducedby means of a volat1le or evaporable carrier is capable ofindurating and toughening porous bodies, such as wood-pulp articles,leather or articles made therefrom, or of toughening and renderingpliable materials such as leather or textiles; and in the case ofleather particularly, of filling, lumping, refining the rain, increasingsoftness and pliability, increasing tensile strength, and, generallyspeaking, so improving the physical characteristics of leather as toraise its grade and market value. Cloth of all kinds and articles madetherefrom can be effectively waterproofed by means of thiscomposition,without suffering any detriment or serious loss of pliability, and withvery little increase in weight. If, on the other hand, increase inweight is a desideratum, the composition may be varied in proportions ofingredients to produce this result.

The general rule to be derived from my demonstrations and observationsis that in order to stiffen and indurate porous material, the resinousingredient should be increased in proportion; while in order to producesoft and pliable products, the crude petrolatum should increaseproportionately. Jrreater or less concentration of both of theseingredients in the solution in the volatile or evaporable carrier willmake. the characteristic eflect more or less marked in the impregnatedproduct.

The mode of compounding this composition of matter and preparing it forintroduction into a porous or bibulous body, which I have adopted inpractice and believe to be the best, is as follows: First, dissolve orout the resinous ingredient in the volatile solvent or carrier.Secondly; add the crude petrolatum and heat the mixture. For suchpurposes as impregnation and induration of wood-pulp articles, or thestiffening and toughening of pliable materials, I have found thefollowing proportions and operations to be suitable: Mix rosin andga'solene in. the proportions of fourpounds of rosin to one gallon ofgasolene (approximately six pounds). When the rosin has been completelydissolved or cut by the gasolene, pour off the clear liquid from suchsediment as may be present, or filter out the. sediment. Then add thecrude petrolatum to the gasolene-rosin solution, using about threepounds ofcrude petrolatum to the gallon of solution, and heat themixture, when the crude petrolatum will also go into solution. The finalproportions ofthe composition made according to this formula will be,approximately, four pounds of rosin, three pounds of crude petrolatumand six pounds of gasolene. If it is intended to produce softer and morepliable articles, as of leather or textile material, the proportions ofrosin and crude petrolatum will be varied; the 4 more preponderant thecrude petrolatum,

the softer and more pliable will be the treated material. DifferentWeights of filler per square or cubic inch of material treated will beobtained by variations in the dilution of the dissolved materials crudepetrolatum and resin) in the volatile carrier.

Porous or bibulous material to be treated with this preparation of thecomposition may be immersed in it, or coated or sprinkled with it,according to the degree of impregnation desired. Preferably thematerials to be treated will be immersed in the preparation of thecomposition, and preferably'also the carrier-liquid and compositionshould be used hot, since heat makes the composite liquid thinner andmore promptly penetrative. If desired, and when the character of theporous material permits, the material to be treated may be heated alsobefore immersion. The carrier with the composition penetrates the porousbody immersed in it,.expelling air from the pores and interstices, andwhen impregnated to the desired degree, the porous body is removed fromthe carrier-bath and dried, either with or without artificial heat, asmay be determined on. The volatile carrier is dissipated, leaving theintimate mixture or composition-of crude petrolatum and resin lodged andfixed in the pores of the material. These, according to the proportionsof the impregnating substances, their quan-v tity per unit of space, andalso according to the physical pecularities of the porous body itself,impart to the product physical characteristics which will be herein moreparticularly illustrated by examples. In all cases, however, theimpregnated bod will be rendered water-proof or water-resistant. Leatherproducts embodying the present invention deserve particular description,since-.they-have properties of marked superiority. I am informed thatalthough many devices have been sought and some resorted to forrendering leather waterproof, that is, impervious to water in the sensethat a rubber sheet is impervious, no permanently water roof leather hasyet been produced. illers or coatings, in themselves impervious towater, such as patent leather finish, are well known; but these, whileprotective as long as they persist unbroken, do not render the leatheritself water-resistant or waterproof. Greasy or oily fillers temporarilyimpart waterresistant properties to leather, but these work out of theleather sooner or later, and leaveit susceptible to water-penetration asbefore.

By impregnating the pores of leather with the composition of crudepetrolatum and a resin, according to my invention, the leather itself,as a sheet of material, becomes permanently waterproof. The crudepetrolatum prevents the leather from becoming stiff or brittle, sincethis filling material is in itself a pliable and softening agent. Alone,it would soon work out of the leather, rendering the surface greasy andliable to spot or grease other objects, and leaving the leather itselfhardly, if at all, more waterproof than originally. The presence of theresin holds and fixes the composition in the. pores of the leather whereit is deposited, as by the evaporation of the solvent or carrier; aresin alone, if deposited in the pores of leather would render theproduct stiff and brittle; the qualifying presence of crude petrolatumprevents this.

The apparatus which I preferably employ in producing the productsclaimed herein isdescribed and claimed in my application Sr. No.247,662, filed on even date herewith. This apparatus comprises a deeptank partially filled with the impregnating composition and arranged tobe heated to a temperature such that the upper portion of the tank isfilled with vapor of the gasolene or other solvent. The hide or skln orother material is dipped into the hot solution and then withdrawnthrough the vapor in the upper portion of the tank. As the hide or skinenters the composition the air is driven out of the pores and thecomposition solution strikes in, thoroughl impregnating the leather. Asthe leat er is drawn out of the composition it is bathed in the vaporwhich occupies the upper part of the tank over the liquid level, andthis vapor-washing removes from the surface of the leather all streaksof greasy material which therwise might remain and degrade the leather.This vapor bath degreases the leather to a slight degree, just enough toclean its surface thoroughly. The leather is then hung up to dry, eitherin the open, or in the drying room.

The physical character of the product depends on the selection ofproportions of ingredients in the treating composition, and

. than ten seconds.

almost any desired variation in result can be obtained after experiencewith, and manipulation of the composition. For instance, to make animproved waterproof leather, use equal parts of crude petrolatum androsin, and an amount of gasolene which weighs about eighty per cent. ofthe com bined weight of the other two ingredients.

If the gasolene is of specific gravity sixty, heat it to 200 F. in thetreating tank and immerse the leather about fifteen seconds. Theproduct, after drying, will be firmer, harder, and less flexible thanthe untreated leather, will be permanently waterproof, much moreresistant to wear, and has a surface susceptible of receiving a highpolish.

If leather for gloves or light shoe up pers is to be produced, say fromcalfskin, use to each gallon of gasolene two pounds of rosin and threepounds of petroleum residue, and treat the leather with this compositionas hot as 200 F. or higher. The leather usually need not be immersedlonger The product is well plumped, the quality and feel of the grainrefined and improved; the leather is soft and flexible, of highertensile strength than originally, and improved in grade. It is, like allproducts thus treated with my composition, completely waterproof. Thistreatment does not seem to affect coloring matter in the leather, butimparts improved character toall kinds of leather without incidentaldetriment. Cemented laminated leather belting can be advantageouslytreated with my composition which imparts the waterproof character tothe belting, increases its tensile strength, decreases its liability tostretching, and ives it a traction surface which requires little or nobelt- 105 dressing.

The vapor bath given to leather on emerging fromthe liquid compositionin apparatus such as above described, is particularly important andbeneficial, since it pre- 1 vents any greasy streaks or exudations fromremaining on the surface of the leather.

As to the treatment of other flexible materials than leather, 1 havewaterproofed cloth garments, tent cloth and miscellane- 115 ous textilearticles, by giving them a single treatment in all essentials like thatabove prescribed for flexible glove or upper leather. I have alsotreated wood pulp articles, using a composition of four pounds 20 ofrosin and three pounds of crude petrolatum to the gallon of gasolene,immersing the wood-pulp articles in the composition at a temperatureabout 200 F., leaving them immersed long enough to insure 125 thoroughpenetration. The product when dry is highly indurated, tough and takesa. high polish. The complete waterproof character of the product adaptssuch im-- pregnated wood-pulp to. a variety of uses. 130

The articles of wood-pulp will be molded to their desired andintendedshape before im regnation.

s a general rule, the higher grades of gasolene, such as commercial 70to 75 s pecific gravity gasolene, form a composltlon which need not beheated to so high a point for good results in treatment of porousbodies. With such gasolene, the temperature need not be much above 150F.

The time of immersion of a body to be impregnated by my new compositionwill depend on the degree of penetration or impregnation desired, thethickness of the body, the degree of fineness of its pores andinterstices, the temperature of the composition, and the degree ofconcentration of soluble ingredients therein. By variations in thesefactors almost any conceivable character or degree of impregnation canbe ob tained.

Both resin and crude petrolatum being inherently water-resistant, acompound of the two, made by heating them together, either with orwithout a diluent, solvent or carrier, is likewise water-resistant. Whenthe pores or interstices of a porous or bibulous body are impregnated bythiscompound, the function of the resin is, in part, to retain thecomposition in the pores or interstices, the crude petrolatum would ofitself tend to work out of the pores or interstices. ,The resin preventsthis and makes the composition, with its greas or lubricant component,stick in the body. he function of the crude petrolatum, in part, is tolubricate, render pliant and tractable, or to toughen rather thanstifi'en, a body, which if impregnated with a resin alone, would bestiff and brittle. The virtues or qualities of one ingredient modify-thetendencies of the other. The composition, while partaking of thequalities of resin and petroleum residue, is neither of these, nor is ita mere aggregation of the two. Each performs its funct on in conjunctionwith that of the other; the joint result is. more than, and differentfrom, an aggregate of the separate results which might be produced bythe use of each separately.

YA composition of these two ingredients may be prepared simply byheating the components together, and each composition, when fluid andhot, will in a measure penetrate the pores or interstices of a porous orbibulous body, and will thus impregnate it. But such a liquidcomposition is not so capable of wetting solid porous bodies as is aliquid such as acts as a solvent or diluent for the impregnatingcomponents. Capillary attraction of the solid body for a liquid is aphysical phenomenon which, as .in the case of gasolene, may be takenadvantage of to secure quick impregnation of a porous body withsubstances which of themselves possess little or inferior capillaryattraction for the body itself. Hence the employment of a liquid diluentor carrier, having capillary attraction for the porous body and beingtherefore capable of promptly wetting it, is a characteristic of thepreferred method above described. Should the impregnation of a porousbody by the impregnating substances themselves, in a liquid state, beresorted to, the surface of the body may be cleansed or washed with asolvent of the impregnating materials either in liquid or vaporouscondition, if it be desired to remove the greasy and resinous substancesfrom the surface.

Themethod above described and the effect of impregnation ofmiscellaneous porous or bibulous bodies with-the new composition ofmatter characterized by crude petrolatum and a resin in intimateassociation with each other, whatever be the specific peculiarity of theporous or bibulous body, or whatever the proportions of the ingredientelements of the composition has this persistent characteristic orquality, that by itthere is produced in the porous or bibulous body aninternal structural continuity of higher degree than is possessed by thebody prior to its treatment with the composition.

This improved or enhanced continuity of substance is responsible for theimperviousness to water which results from impregnation, in conjunctionwith the water-repellent or resistant properties inherent in theimpregnating composition itself. Enhanced continuity is consistent, alsowith the increase in toughness produced in bodies indurated with thecomposition in which resin predominates, as well as with the improvedsmoothness and pliability of' other bodies, impre nated with thecomposition in which the In ricant crude petrolatum predomi' nates.

I claim:

1. Porous material having its porosities impregnated with a compositioncomposed essentially of crude petrolatum and a resin.

2. Porous material having its porosities impregnated with a compositioncomposed essentially of crude petrolatum and colophony.

3. An article of manufacture comprising leather impregnated with acomposition composed essentially of crude petrolatum and a resin.

4. An article of manufacture comprising leather impregnated with acomposition composed essentially of crude petrolatum and colophony.

5. An article of manufacture comprising leather impregnated with anon-parafiinic composition composed essentially of crude petrolatum anda resin.

' 6. An article of manufacture comprising composition composedessentially of crude petrolatum and colophony.

7. An article of manufacture comprising porous material impregnated witha composition comprising crude petrolatum.

8. An article of manufacture comprising porous material impregnated witha'composition comprising crude petrolatum and a resin.

9. An article of manufacture comprising porous material impregnated witha composition comprising crude petrolatum and colophony. 7

10. An article of manufacture comprising porous material impregnatedwith a composition comprising crude petrolatum in major art.

11. 11 article of manufacture comprising porous material impregnatedwith a composition comprising crude petrolatum and a resin in which theformer predominates.

12. An article of manufacture comprising leather impregnated with acomposition comprising crude petrolatum.

13. An article of manufacture comprising leather impregnated with acomposition comprising crude etrolatum and a resin.

14. An article 0 manufacture comprising leather impregnated with acomposition comprising crude, petrolatum and colophony.

15. An article of manufacture comprising leather impregnated with acomposition comprising crude petrolatum in major part.

16. An article of manufacture comprising leather impregnated with acomposition comprising crude petrolatum and a resin, the amount of crudepetrolatum being at least of the order of the amount of resin.

17 An article of manufacture comprising leather impregnated with acomposition comprising crude petrolatum and a resin in which the formerpredominates.

18. An article of manufacture comprising porous material impregnatedwith a nonparaflinic composition comprising crude petrolatum. i

19. An article of manufacture comprising porous material impregnatedwith a nonparaffin'ic composition comprising crude petrolatum and aresin.

20. An article of manufacture comprising porous material impregnatedwith a nonparaflinic composition comprising crude petrolatum andcolophony. I

21. An article of manufacture comprising porous material impregnatedwith a nonparafiinic composition comprising crude pet rolatum in majorpart.

22. An article of manufacture comprising porous material impregnatedwith a nonparaflinic composition comprising crude petrolatum and a resinin which the former predominates.

Signed by me at Boston, Massachusetts, this 25th day of April, 1918.

WINTWORTH V. LANDER.

